Acetic Anhydride → HCID 1482611, compound

Participants

Reaction Steps

A mixture of ethyl 4,4,4-trifluoroacetoacetate (3.59 g, 19.5 mmol), ethyl orthoformate (4.49 mL, 27 mmol) and acetic anhydride (5.10 mL, 54 mmol) was heated under reflux for 3.5 hr, and the mixture was concentrated under reduced pressure. Ethanol (50 mL) and thiosemicarbazide (1.37 g, 15 mmol) were added, and the reaction mixture was stirred at room temperature for 2.5 hr. 2-Bromo-1-(3,4-dichlorophenyl)ethanone (4.02 g, 15 mmol) was added, and the mixture was stirred at 80° C. for 30 min, cooled to room temperature. The precipitated crystals were collected by filtration to give a crude title compound (4.73 g, 72%) as colorless crystals.

Provenance & Evidence